反応 #1791507

ord-43af29c1327347f688da3bc820bab4dc

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    ろ過was filtered
  3. 3
    workup.ADDITIONA drop of concentrated hydrochloric acid was added to the filtrate which
  4. 4
    その他removed some color
  5. 5
    その他to yield a cream color material
  6. 6
    その他Recrystallization from toluene
  7. 7
    その他gave needles, (93% yield)
  8. 8
    その他sintered at 177° C.

実験手順

A stirred solution of 9 g. (0.028 mole) of 7-(4-chlorobenzoyl)-3-methylthioindolin-2-one in 180 ml. of tetrahydrofuran was treated over a two-hour period with 45 g. of a commercial Raney nickel water suspension. After the addition was complete the mixture was filtered. A drop of concentrated hydrochloric acid was added to the filtrate which removed some color and the resulting solution was then stripped under water pump vacuum to yield a cream color material. Recrystallization from toluene gave needles, (93% yield); the material sintered at 177° C. and melted at 186° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04126635uspto-grants-1978_11